Acetic Anhydride → 2-(2-Acetoxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

HRID 544664ノート

反応式

HRID 544664 の反応式
[OH:1][CH2:2][CH2:3][S:4][C:5]1[S:6][C:7]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[N:9]=1.[C:26](OC(=O)C)(=[O:28])[CH3:27]>>[C:26]([O:1][CH2:2][CH2:3][S:4][C:5]1[S:6][C:7]([C:18]2[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=2)=[C:8]([C:10]2[CH:11]=[CH:12][C:13]([O:16][CH3:17])=[CH:14][CH:15]=2)[N:9]=1)(=[O:28])[CH3:27]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 132096672-(2-Hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

生成物 1

HCID 204583632-(2-Acetoxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

実験手順

5.0 g of 2-(2-hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole are suspended in 50 ml of acetic anhydride and, while stirring, the suspension is heated to the boil and refluxed for 15 minutes. The product is concentrated to dryness by evaporation under reduced pressure, two 30 ml portions of xylene are added, with concentration by evaporation being carried out again after each addition to remove traces of acetic anhydride, and the residue is dried under reduced pressure. 2-(2-Acetoxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole is obtained in the form of an oil, Rf =0.33 (silica gel toluene/ethyl acetate 10:1), IR-spectrum: νC=O =1730 cm-1 (CCl4).

後処理

  1. temperaturethe suspension is heated to the boil
  2. temperaturerefluxed for 15 minutes
  3. concentrationThe product is concentrated to dryness by evaporation under reduced pressure, two 30 ml portions of xylene
  4. additionare added, with concentration by evaporation
  5. additionafter each addition
  6. customto remove traces of acetic anhydride
  7. customthe residue is dried under reduced pressure

出典と根拠

ORDレコード
ord-e477768b3a92435bbd60403c66f39988
出典データセット
uspto-grants-1984_05
特許番号
US04451471

反応ノート

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